摘要
分别利用微乳液水热法和酸蒸气水热法合成了杂多蓝化合物 Zr W 1 .7W 0 .3O7H0 .3( OH) 2 · 2 H2 O.XRD测定结果表明 ,该化合物与 Zr Mo2 O7( OH) 2 · 2 H2 O具有相同晶体结构类型 .使用 Rietveld方法对产物进行了结构精修 ,并计算出了键参数和键价 .运用 EPR技术测定了该化合物中 W的价态 ,并利用 XPS能谱测定了 W /W 的比例 .利用价键和规则 ,指出 Zr W 1 .7W 0 .3O7H0 .3( OH) 2 · 2 H2 O中的 W— O3— H0 .1 5存在羟基化现象 ,并对杂多蓝化合物的红外吸收光谱进行了指认 .
A new sort of heteropoly blue compound,ZrW Ⅵ_ 1.7 W Ⅴ_ 0.3 O_7H_ 0.3 (OH)_2 ·2H_2O,was synthesized by the acidic-steam hydrothermal process and the microemulsion hydrothermal process. XRD pattern proves that the heteropoly blue compound has the same type of crystal structure as that of ZrMo_2O_7(OH)_2· 2H_2O. The rietveld refinement method was used to refine the crystal structure of the heteropoly blue compound. The bond parameters were calculated and the bond valences of atoms were obtained. The EPR result affirmed the subsistence of W Ⅴ ion in the new compound,and the molar ratio of W Ⅴ/W Ⅵ was determined by XPS. Combining with bond valences of atoms and IR spectra analysis,random hydroxylation of W—O3—H_ 0.15 exits in the molecule and the FTIR absorption spectra were assigned. [WT5HZ]
出处
《高等学校化学学报》
SCIE
EI
CAS
CSCD
北大核心
2004年第6期1005-1009,共5页
Chemical Journal of Chinese Universities
基金
国家自然科学基金 (批准号 :2 98710 0 6
2 0 13 3 0 3 0 )
北京市无机化学重点学科项目资助
